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WO1997042125A1 - Particule de magnetite ultra fine noire et leur procede de preparation - Google Patents

Particule de magnetite ultra fine noire et leur procede de preparation Download PDF

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Publication number
WO1997042125A1
WO1997042125A1 PCT/JP1997/001524 JP9701524W WO9742125A1 WO 1997042125 A1 WO1997042125 A1 WO 1997042125A1 JP 9701524 W JP9701524 W JP 9701524W WO 9742125 A1 WO9742125 A1 WO 9742125A1
Authority
WO
WIPO (PCT)
Prior art keywords
black
magnetite
magnetite particles
ultrafine
particles
Prior art date
Application number
PCT/JP1997/001524
Other languages
English (en)
Japanese (ja)
Inventor
Naoyoshi Mochizuki
Kenzo Hanawa
Original Assignee
Mitsui Mining & Smelting Company, Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mitsui Mining & Smelting Company, Ltd. filed Critical Mitsui Mining & Smelting Company, Ltd.
Priority to JP53974197A priority Critical patent/JP3464801B2/ja
Priority to US08/981,332 priority patent/US6083476A/en
Publication of WO1997042125A1 publication Critical patent/WO1997042125A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C01G49/08—Ferroso-ferric oxide [Fe3O4]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/22—Compounds of iron
    • C09C1/24—Oxides of iron
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/42—Magnetic properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
    • Y10T428/2995—Silane, siloxane or silicone coating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
    • Y10T428/2996—Glass particles or spheres
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2998—Coated including synthetic resin or polymer

Definitions

  • the present invention relates to black ultrafine magnetite particles mainly used for magnetic toner material powder for electrostatic copying and black pigment powder for paint, and a method for producing the same.
  • magnetite Since the magnetite currently used has a particle size of 0.1 to 0.3 // m, the necessity of ultrafine magnetite having a particle size of 0.1 m or less is increasing. However, there are currently no magnetite ultrafine particles of 0.1 m or less that have a black tint that can be used as a black pigment.
  • the magnetite fine particles used for magnetic black pigment in magnetic toner are generally sulfuric acid. Alkali is added to ferrous iron to obtain a suspension of Fe (OH) 2, and the magnetite particles obtained by air oxidation at an appropriate temperature are used. PH, oxidation rate, reaction temperature, etc.
  • Various studies have been made to obtain fine particles of 0.1 m or less by examining the above conditions, but it is difficult to reduce the size to less than 0.1 m while maintaining black.
  • the water content is reduced to less than 0.01 m. It is well known that ultrafine magnetite can be produced.
  • the ultrafine particles obtained in this way are too fine to be oxidized when taken out into the air, making it difficult to use them in applications such as magnetic toners, and are taken out into the air like magnetic fluids. Is limited to uses that do not.
  • Japanese Patent Publication No. 2-336555 discloses an ultrafine magnetite of about 0.01 to 0.025 m. Is disclosed.
  • the ferrous salt is increased in proportion to the composition of the magnetite.
  • This ferrous hydroxide is air-oxidized to grow the magnetite by air oxidation on the coprecipitated ultrafine magnetite particles to make the ultrafine magnetite somewhat larger. It is a way to stabilize.
  • the present invention provides a black super- It is an object to provide fine magnetite particles and a method for producing the same. Disclosure of the invention
  • Magunetai preparative chemical composition is represented by F e O 'F e 2 0 3, the original F e ⁇ weight of 3 1%.
  • F e O 'F e 2 0 3 the original F e ⁇ weight of 3 1%.
  • oxidation tends to proceed, and it is difficult to maintain the Fe 0 content at 31% when actually taken out into the air.
  • the grain size of Magunetai bets particles are used as the black magnetic pigment, 0. 1 ⁇ 0. 3 m, although the BET specific surface area is of 2 ⁇ 1 O m 5 / g , F e ⁇ Is not about 31% but about 20 to 26% c
  • the conventional particle size is controlled at about 25%, it is possible to obtain a magnet with blackness that can be used as a black pigment, but as the particle size becomes smaller, Fe 0 It turned out that the reddish color increased even if the amount of the same.
  • Black ultrafine magnetite particles based on such findings are characterized by a Fe 0 content of 31 to 35% and a particle size of 0.1 m or less, and a small particle size.
  • the specific surface area increases, the specific surface area increases, and oxidation tends to occur. Therefore, the amount of Fe 0 tends to decrease as the particle size decreases.
  • FeO decreased. It gets a little worse as it gets smaller.
  • the particle size is large, the particles are polycrystalline and are absorbed during repetition of refraction.As a result, the particles become black, but as the particle size becomes smaller, the particle size becomes smaller. Since refraction can no longer be expected, the absorption characteristics of the particles themselves are directly effective.
  • the amount of 60 is 10 to 20%.
  • a method for controlling the amount of FeO is described in Japanese Patent Publication No. 51-9718. That is, the magnetite particles are dispersed in water containing ferrous hydroxide, and alkali is added so that the pH of the dispersion is 8.0 to 14 and the temperature is 50 to 100 ° C. Ripen in a non-oxidizing atmosphere.
  • F e O x ⁇ F e 2 0 3 and has a 0 rather X rather 1 when displayed is the amount force 3 1%
  • F e O in-out x l Noto force, et
  • the amount of FeO is less than 31%. Therefore, magnetite particles with a Fe 0 force of 31% or more can be considered as a completely new substance as compared with conventional magnetite particles.
  • ferrous hydroxide slurries with a pH of 14 or more, that is, free alcohol of 1 mol Z liter (MZ) or more, among 90 to 10 It was found that the amount of FeO can be increased to 31% or more when aged at a temperature of 0 ° C. It was also found that the limit was 35%, and that the amount of Fe0 could not be further increased. At this time, it is not necessary to make the atmosphere non-oxidizing. The amount of ferrous hydroxide to be added penetrates the magnetite up to 35% Fe 0, but remains as ferrous hydroxide beyond that.
  • ferrous hydroxide If it is left as ferrous hydroxide, it will be extremely difficult to clean and dry. Further, after drying, ferrous hydroxide is very susceptible to oxidation, and even if it is subjected to an antioxidant treatment. It usually burns when taken out into the air after drying. Therefore, the amount of ferrous hydroxide added must be strictly controlled so that the final Fe 0 content falls between 31 and 35%.
  • sodium oleate is added to the suspension, and the pH is adjusted to 5 to 6, so that oleic acid is deposited on the surface of the magnetite. Can be done. After that, wash 'filtration' and dry.
  • sodium oleate may be added after washing the by-produced sodium sulfate after the FeO addition treatment. However, sodium oleate does not dissolve well unless the pH is 8 or higher.
  • the amount of sodium oleate added to the magnetite particles is preferably 0.2 to 5%.
  • the antioxidant effect is not sufficiently exhibited.
  • the amount exceeds 5%, the magnetite fine particles are heavily agglomerated with oleic acid and the toner This is because they cannot be mixed with the resin at the same time and are not preferred together.
  • a potassium phosphate of oleic acid may be used.
  • a method for producing black ultrafine magnetite particles based on such findings is to disperse ultrafine magnetite of 0.1 m or less in water containing ferrous hydroxide, and to increase the alkalinity of free to 1 mol. / Little (M / ⁇ ) or more and aged at 90-i00 ° C, and then sodium oleate or potassium oleate is added to the magnetite particles for 0.2-5 % And adjust the pH to 5 to 6 to deposit oleic acid on the magnet. It is characterized by BEST MODE FOR CARRYING OUT THE INVENTION
  • the saturation magnetization of the fine particle magnet powder was 83 emu / g, the BET specific surface area was 43 m 2 Z g, and the analysis result of Fe 0 was 17%.
  • 50 g of the above particulate magnetite powder was mixed with 50 g of low molecular weight polyethylene wax at 150 ° C for 1 hour with a biaxial nigo for 1 hour, and the mixture was taken out. It was pulverized to 1 mm or less, further pulverized with a jet mill to an average particle diameter of 10 m, and the color tone of the resin mixture having a particle diameter corresponding to the toner was observed.
  • the fine magnetite powder was black, but the one mixed with resin had a strong reddish color.
  • the saturation magnetization was 84 emu Zg
  • the BET specific surface area was 25 m 2 / g
  • the analysis result of F e O was 32%.
  • Table 1 shows the results of examining the saturation magnetization, BET specific surface area, amount of FeO, and color tone after mixing with the resin of the black powder.
  • the saturation magnetization was 83 emu Zg
  • the BET specific surface area was 13 m 2 Zg
  • the analysis result of F e 0 was 33%.
  • the mixture was mixed with the resin and the color tone was examined in the same manner as in the example.
  • the following treatment was performed using ultrafine magnetite having a BET specific surface area of 43 m 2 Zg used in the first embodiment.
  • the following treatment was performed using the ultrafine magnetite having a BET specific surface area of 43 m 2 / g used in the first embodiment.
  • the saturation magnetization is 82 emu and the BET specific surface area is 27 m 2 / g F
  • the analysis result of e 0 was 27%.
  • the following treatment was performed using the ultrafine magnetite having a BET specific surface area of 43 m 2 / g used in the first embodiment.
  • the saturation magnetization was 81 emu / g
  • the BET specific surface area was 38 m 2 / g
  • the analysis result of Fe 0 was 25%.
  • the particles do not become reddish even when the particles are taken out into the air, and can be made by conventional technology as a black pigment with ultrafine magnetite of 0.1 m or less. It is possible to obtain black ultrafine magnetite particles that can maintain the black color even when mixed with resin for black magnetic toner.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Composite Materials (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Iron (AREA)
  • Developing Agents For Electrophotography (AREA)

Abstract

L'invention concerne des particules de magnétite ultra fine noire présentant une teneur en FeO comprise entre 31 et 35 % et un diamètre particulaire non supérieur à 0,1 νm, et un procédé de préparation desdites particules consistant à disperser des particules de magnétite ultra fine d'un diamètre n'excédant pas 0,1 νm dans de l'eau contenant de l'hydroxyde ferreux, à laisser venir à maturation la dispersion dans des conditions de teneur en alcali libre non inférieur à 1 mol/l (M/l) entre 90 et 100 °C, ensuite à ajouter de l'oléate de sodium ou de l'oléate de potassium en une quantité comprise entre 0,2 et 5 % sur la base des particules de magnétite, et à ajuster le pH du mélange entre 5 et 6 afin de revêtir les particules de magnétite d'acide oléique.
PCT/JP1997/001524 1996-05-08 1997-05-07 Particule de magnetite ultra fine noire et leur procede de preparation WO1997042125A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP53974197A JP3464801B2 (ja) 1996-05-08 1997-05-07 黒色超微粒マグネタイト粒子およびその製造方法
US08/981,332 US6083476A (en) 1996-05-08 1997-05-07 Black ultrafine magnetite particles and process for preparing the same

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP8/113397 1996-05-08
JP11339796 1996-05-08

Publications (1)

Publication Number Publication Date
WO1997042125A1 true WO1997042125A1 (fr) 1997-11-13

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PCT/JP1997/001524 WO1997042125A1 (fr) 1996-05-08 1997-05-07 Particule de magnetite ultra fine noire et leur procede de preparation

Country Status (3)

Country Link
US (1) US6083476A (fr)
JP (1) JP3464801B2 (fr)
WO (1) WO1997042125A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015052116A (ja) * 2006-05-18 2015-03-19 ランクセス・ドイチュランド・ゲーエムベーハー 酸化安定性酸化鉄顔料、その調製方法、およびその使用

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6962685B2 (en) * 2002-04-17 2005-11-08 International Business Machines Corporation Synthesis of magnetite nanoparticles and the process of forming Fe-based nanomaterials
CN100453469C (zh) * 2006-12-30 2009-01-21 中国科学技术大学 一种赤铁矿纳米立方体的制备方法
JP5784292B2 (ja) * 2010-09-13 2015-09-24 三井金属鉱業株式会社 マグネタイト粒子

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JPS4935520B1 (fr) * 1970-10-20 1974-09-24
JPH07257930A (ja) * 1994-03-22 1995-10-09 Mitsubishi Materials Corp 球状マグネタイト粒子およびその製造方法
JPH0834617A (ja) * 1994-07-22 1996-02-06 Toda Kogyo Corp 黒色磁性酸化鉄粒子粉末

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JPS4935520B1 (fr) * 1970-10-20 1974-09-24
JPH07257930A (ja) * 1994-03-22 1995-10-09 Mitsubishi Materials Corp 球状マグネタイト粒子およびその製造方法
JPH0834617A (ja) * 1994-07-22 1996-02-06 Toda Kogyo Corp 黒色磁性酸化鉄粒子粉末

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015052116A (ja) * 2006-05-18 2015-03-19 ランクセス・ドイチュランド・ゲーエムベーハー 酸化安定性酸化鉄顔料、その調製方法、およびその使用

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US6083476A (en) 2000-07-04
JP3464801B2 (ja) 2003-11-10

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